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EP3671179B1 - Optischer teilchendetektor - Google Patents

Optischer teilchendetektor Download PDF

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Publication number
EP3671179B1
EP3671179B1 EP19218622.9A EP19218622A EP3671179B1 EP 3671179 B1 EP3671179 B1 EP 3671179B1 EP 19218622 A EP19218622 A EP 19218622A EP 3671179 B1 EP3671179 B1 EP 3671179B1
Authority
EP
European Patent Office
Prior art keywords
optical
channel
angular
photodetector
angular filtering
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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Application number
EP19218622.9A
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English (en)
French (fr)
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EP3671179A1 (de
Inventor
Gabriel JOBERT
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Commissariat a lEnergie Atomique et aux Energies Alternatives CEA
Original Assignee
Commissariat a lEnergie Atomique CEA
Commissariat a lEnergie Atomique et aux Energies Alternatives CEA
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
    • G01N15/02—Investigating particle size or size distribution
    • G01N15/0205—Investigating particle size or size distribution by optical means
    • G01N15/0211—Investigating a scatter or diffraction pattern
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
    • G01N15/06—Investigating concentration of particle suspensions
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
    • G01N15/10—Investigating individual particles
    • G01N15/14—Optical investigation techniques, e.g. flow cytometry
    • G01N15/1434—Optical arrangements
    • G01N15/1436—Optical arrangements the optical arrangement forming an integrated apparatus with the sample container, e.g. a flow cell
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
    • G01N15/10—Investigating individual particles
    • G01N15/14—Optical investigation techniques, e.g. flow cytometry
    • G01N15/1456—Optical investigation techniques, e.g. flow cytometry without spatial resolution of the texture or inner structure of the particle, e.g. processing of pulse signals
    • G01N15/1459—Optical investigation techniques, e.g. flow cytometry without spatial resolution of the texture or inner structure of the particle, e.g. processing of pulse signals the analysis being performed on a sample stream
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
    • G01N33/0004—Gaseous mixtures, e.g. polluted air
    • G01N33/0009—General constructional details of gas analysers, e.g. portable test equipment
    • G01N33/0027—General constructional details of gas analysers, e.g. portable test equipment concerning the detector
    • G01N33/0036—General constructional details of gas analysers, e.g. portable test equipment concerning the detector specially adapted to detect a particular component
    • G01N33/0057—Warfare agents or explosives
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
    • G01N33/18—Water
    • G—PHYSICS
    • G08—SIGNALLING
    • G08B—SIGNALLING OR CALLING SYSTEMS; ORDER TELEGRAPHS; ALARM SYSTEMS
    • G08B17/00—Fire alarms; Alarms responsive to explosion
    • G08B17/10—Actuation by presence of smoke or gases, e.g. automatic alarm devices for analysing flowing fluid materials by the use of optical means
    • G08B17/103—Actuation by presence of smoke or gases, e.g. automatic alarm devices for analysing flowing fluid materials by the use of optical means using a light emitting and receiving device
    • G08B17/107—Actuation by presence of smoke or gases, e.g. automatic alarm devices for analysing flowing fluid materials by the use of optical means using a light emitting and receiving device for detecting light-scattering due to smoke
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
    • G01N15/06—Investigating concentration of particle suspensions
    • G01N15/075—Investigating concentration of particle suspensions by optical means
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/47—Scattering, i.e. diffuse reflection
    • G01N2021/4704—Angular selective
    • G01N2021/4711—Multiangle measurement
    • G01N2021/4716—Using a ring of sensors, or a combination of diaphragm and sensors; Annular sensor

Definitions

  • the present invention relates to the field of optical detection of particles in general and more particularly of particles of micrometric or even nanometric size. It also relates to the angular analysis of the diffusion of one or more particles.
  • Particles are microscopic solid, liquid or wet solid objects suspended in the air. Their sizes vary from a few tens of nanometers to a few tens of micrometers. These particles come from various sources such as forest fires, construction sites, industrial sites, motor vehicles etc.
  • the concentration of these particles exceeds a certain threshold, they have a harmful impact on the environment and/or health.
  • some states have set maximum concentration thresholds.
  • the European Union allows maximum concentrations of 50 ⁇ g/m3 for particles between 10 ⁇ m and 2.5 ⁇ m and 25 ⁇ g/m3 for particles less than 2.5 ⁇ m.
  • Different particle detection methods exist, such as gravimetric detection methods, ionization detection methods, beta attenuation detection methods, aerodynamic mobility or electric mobility measurement detection methods, optical detection methods.
  • Optical detection of particles is generally done by means of a device comprising a light source, which illuminates a channel through which the particles to be detected pass, and at least one photodetector.
  • particles If particles are present in the illuminated area, they will absorb part of the light coming from the source and will deflect another part of this light away from the main direction of propagation, according to the phenomenon of diffusion.
  • a first method of optical detection therefore consists of measuring the absorption of light through a cloud of particles or an accumulation of particles. This measurement makes it possible to determine the concentration of particles using the Beer-Lambert law if the composition of the particle cloud is known a priori.
  • a second method is to analyze the light scattered off the optical axis.
  • Angular analysis of the scattered light from the recording of an angular radiation pattern, allows the shape, size, optical index and concentration of particles to be determined.
  • the size, refractive index and concentration of particles can be determined from light scattering theories, for example the Mie theory (Ref: Bohren and Huffmann, Absorption and scattering of light by small particles, Ed. Wiley and Sons, 1983 ).
  • a device comprising a goniometer consisting of a photodetector mounted on a rotating arm, or a device comprising a discrete assembly of photodetectors distributed outside the optical axis.
  • Angular analysis by a device comprising a goniometer has the disadvantages of being very complex, very expensive and not very robust. Thus, it cannot be easily transported. Furthermore, it cannot be considered for equipping low-cost alarm or measurement systems. However, for example, for the field of fire detection in homes or for the field of air quality control, it is essential to offer solutions whose costs are low and whose robustness is high.
  • the document FR3062209 A1 describes another solution for performing an angular analysis. This solution is based on a device comprising a discrete assembly of photodetectors forming a matrix as well as reflective surfaces to project onto the matrix the image of the radiation scattered by the particles. In practice, it turns out that this solution generates an angular blur on the angular radiation diagram.
  • This solution also generates measurement noise on the angular diagram.
  • the present invention aims to at least partially overcome the drawbacks cited above.
  • An object of the present invention is an optical particle detector making it possible to obtain an angular radiation pattern while limiting angular blur.
  • Another object of the present invention is an optical particle detector making it possible to obtain an angular radiation pattern while limiting the measurement noise.
  • the detector further comprises an angular filtering system comprising a plurality of angular filtering devices each associated with a photodetector, each angular filtering device being configured to angularly filter the light rays coming from the channel before their reception by the photodetector with which it is associated.
  • Each photodetector thus benefits from its own angular filtering device.
  • Each photodetector receives only a part of the light rays coming from the channel, this part being included in a region limited by limiting angles of incidence of the light rays, defined by the angular filtering device of the photodetector.
  • This region limited by the limiting angles of incidence corresponds to the collection cone of the angular filtering device.
  • This collection cone 40 as well as the principle of angular filtering is illustrated in figure 1 .
  • the angular blur observed in the detectors of the prior art is notably due to parasitic diffusions which are generated by the presence of several particles. 10, 10' in channel 1 or by the variation of position of a diffusing particle in channel 1.
  • the light ray iii of the particle 10' remains outside the collection cone 40 of the angular filtering device 431 associated with the photodetector 33. This light ray iii is therefore never detected by the photodetector 33, although the particle 10' is present in the channel. It is then possible to analyze with significantly improved precision the particle 10 whose light ray ii enters the collection cone 40 and reaches the photodetector 33.
  • the angular blur of the photodetector is advantageously limited thanks to the angular filtering device of the present invention.
  • the angular blur observed with prior art detectors may also arise from the variation in position of a scattering particle in channel 1.
  • a particle 10 diffuses, when it is located in an initial position, for example a light ray ii and a light ray iii.
  • the light ray ii is included in the collection cone 40 of the angular filtering device 431 associated with the photodetector 33. It is therefore detected by the photodetector 33.
  • the light ray iii is outside the collection cone 40 of the angular filtering device 431 associated with the photodetector 33. It is not detected by the photodetector 33.
  • the light ray iii advantageously remains outside the collection cone 40 of the angular filtering device 431 associated with the photodetector 33.
  • the light ray iii is therefore never detected by the photodetector 33, although the particle has moved.
  • the angular blur of the photodetector is advantageously limited thanks to the angular filtering device of the present invention.
  • Another source of parasitic detection comes from light rays iv scattered indirectly, for example by an edge of the channel 1 or by a protective layer, for example an encapsulant of the photodetectors. These indirect light rays iv are also detected by the photodetectors of the detectors of the prior art. They then generate measurement noise in the angular analysis of the rays scattered by the particle 10.
  • the light rays iv advantageously remain outside the collection cone 40 of the angular filtering device 431 associated with the photodetector 33. These light rays iv are therefore never detected by the photodetector 33.
  • the measurement noise of the photodetector is advantageously limited thanks to the angular filtering device of the present invention.
  • the present invention has a particular advantage for detectors in which a channel or an encapsulation layer inevitably generates parasitic diffusions.
  • the light rays coming from the channel are advantageously collected selectively by an angular filtering device, depending on their angles of incidence and the position of their emission or re-emission source, provided that they are located in the collection cone of the angular filtering device considered.
  • the detector according to the invention can have at least some of the optional characteristics set out below which can possibly be used in combination or alternatively.
  • Each angular filtering device preferably comprises an optical input having a numerical aperture of less than 0.3, preferably less than 0.2, and preferably of the order of 0.1.
  • the numerical aperture is proportional to the half-opening angle y, corresponding to the limiting angle of incidence, relative to the optical axis of the input of the angular filtering device considered, beyond which a light ray is no longer collected by this input.
  • a numerical aperture of less than 0.3 corresponds to a half-opening angle ⁇ of less than approximately 17°.
  • An angular filtering system comprising such angular filtering devices therefore advantageously makes it possible to limit, or even eliminate, parasitic diffusion, i.e. diffusion comprising rays indirectly diffused iv by elements other than the particle(s).
  • the collection at an entrance of a ray directly scattered by a particle implies that this particle is located in the collection cone defined by the numerical aperture of said entrance of the angular filtering device.
  • Such an angular filtering system therefore advantageously makes it possible to limit angular blur.
  • Numerical aperture is a characteristic of an optical system, generally noted NA according to the Anglo-Saxon terminology for "Numerical Aperture”.
  • NA n 0 .sin i 0 , where n 0 is the refractive index in the observation medium, and i 0 is the angle between the optical axis of the optical system and the ray most inclined to the optical axis, which exits from or enters the optical system. This angle is called the half-opening angle.
  • ⁇ 2.i 0 the opening angle.
  • LED light-emitting diodes which are not very directional, have significantly larger numerical apertures than laser diodes, which are very directional.
  • NA is a characteristic specific to the guiding structure. It appears that by decreasing the index contrast, that is to say the difference between these two indices n c and n g , the numerical aperture NA decreases.
  • the collection cone of the guiding structure is a function of the numerical aperture.
  • a collection cone is understood to mean a beam of light rays, in particular scattered light rays, admissible by the optical system.
  • the collection cone does not necessarily have a circular base or axial symmetry.
  • the collecting cone may, for example, have an elliptical base or a rectangular base.
  • particle or its equivalents is defined as a constituent of a physical system considered as elementary in relation to the properties studied.
  • particles refers in particular to a solid, liquid or wet solid object suspended in the air and whose size is microscopic.
  • a particle is an element of matter whose largest dimension is less than a few millimeters (10 -3 meters), preferably one millimeter, and preferably a few tens of micrometers (10 -6 meters) and preferably less than a micrometer, or even of the order of a nanometer (10 -9 m). More generally, particles have a size greater than 40 ⁇ (10 -10 m) and are therefore considered optically continuous. Generally speaking, these are objects composed of matter whose dimensions are small compared to the dimensions of the cavity or the particle circulation channel.
  • the "size” or “diameter” of a particle is the maximum distance between two points on the particle.
  • a particle is thought of as an object of spherical geometry, so its size corresponds to the diameter of the sphere.
  • a substrate, waveguide, film, layer, "based" on a material A means a substrate, waveguide, film, layer comprising this material A only or this material A and possibly other materials, for example doping elements or alloying elements.
  • a waveguide is designated as being "polymer-based", this means that it can be formed only of polymers or of polymers and possibly other materials, for example an inorganic oxide.
  • the term “on”, “overcomes”, “covers” or “underlying” or their equivalents do not mean “in contact with”.
  • the deposition of a first layer on a second layer does not necessarily mean that the two layers are directly in contact with each other, but it does mean that the first layer at least partially covers the second layer by being either directly in contact with it or by being separated from it by at least one other layer or at least one other element.
  • the term “absorption” or its equivalents refers to the phenomenon by which the energy of an electromagnetic wave is transformed into another form of energy, for example in the form of heat.
  • a material is considered to be absorbent when it absorbs at least 50% of light radiation, preferably at least 75% and advantageously at least 90%. It can be characterized by an absorption factor between 0 and 1.
  • the term "diffusion” or its equivalents refers to the phenomenon by which a propagation medium produces a distribution, in many directions, of the energy of an electromagnetic wave, light for example.
  • the term “reflection” or its equivalents refers to the phenomenon of re-emission from an element or a surface of an incident light radiation.
  • an element is considered to be reflective when it re-emits at least a portion of an incident light radiation, this portion being greater than or equal to 50%. It can be characterized by a reflection factor between 0 and 1.
  • a direction substantially normal to a plane means a direction having an angle of 90 ⁇ 5° with respect to the plane.
  • the present invention finds as its preferred field of application the detection of particles of various sizes, preferably in the field of microscopic or even nanometric particles.
  • the present invention can be used for the detection of particles from smoke, explosive powder, pollutant particles, dust particles, allergen particles such as pollen, mold spores, or even carcinogenic particles, or biological particles such as bacteria, viruses, or even exosomes.
  • the present invention applies to any type of particles carried by a fluid, whether liquid and/or gaseous.
  • the fluid present or flowing in the channel is for example air.
  • a fire alarm system a fire detection system, an explosive powder detection system, a system for analyzing the quality of a fluid such as air, an anti-pollution alarm system.
  • the fluid may be a liquid such as water. This is the case for detectors integrated into microbiological species detection systems.
  • the present invention aims in particular to carry out angularly resolved diffusion measurements of one or more particles within a detector manufactured using conventional micro-fabrication technologies.
  • the detector comprises a channel 1 in which a fluid comprising at least one particle 10 can circulate and a detection system 3 comprising a plurality of photodetectors 31, 32, 33 intended to collect scattered light rays ii.
  • This plurality of photodetectors may comprise at least seven photodetectors, preferably at least twelve photodetectors, and preferably a number of photodetectors greater than twelve, so that the detector can perform sufficiently complete angular sampling.
  • the angular resolution of the detector can be increased by increasing the number of photodetectors.
  • the detector is coupled to an optical source 2.
  • the source 2 is preferably separate from the detector. This allows the source to be changed or manufactured independently of the detector.
  • the detector further comprises an angular filtering system 4 configured to filter the collection of the scattered light rays ii according to certain scattering angles only.
  • an angular filtering system 4 configured to filter the collection of the scattered light rays ii according to certain scattering angles only.
  • Such a system 4 makes it possible to reduce the measurement noise due to parasitic scatterings which do not directly originate from the particle 10.
  • Such a system 4 also makes it possible to reduce the angular blur generated by the movement of the particle 10, 10'.
  • This system 4 also makes it possible to reduce the angular blur generated by the scattering on the same photodetector, for example the photodetector 33, of rays scattered simultaneously by several particles 10, 10' present in the channel (the references 10, 10' refer either to two different positions of the same particle, or to two distinct particles, for the sake of brevity).
  • These elements are for example a crown, a barrel or a support plate hollowed out in its center allowing the fluid to flow into channel 1.
  • the channel 1 is preferably cylindrical.
  • the circulation of the fluid is mainly along the longitudinal axis of this channel.
  • this axis is perpendicular to the plane of the sheet.
  • This channel can have a transverse dimension, for example a diameter, between 100 ⁇ m and 3 mm.
  • the emission of incident light rays i and the collection of scattered light rays ii are preferably carried out in a plane transverse to the longitudinal axis of this channel 1.
  • the emission of incident light rays i takes place at an optical output 21 associated with a light source 2.
  • the source 2 can be associated with a device for forming an incident beam 22 configured to transmit incident light rays i included in an illumination cone 20 extending from the optical output 21.
  • This incident beam forming device 22 may be a guiding structure such as a waveguide, an optical fiber, a light trap or a microlens system for example.
  • the optical output 21 therefore has a numerical aperture NAi allowing the emission of only the incident light rays i included in its illumination cone 20.
  • the numerical aperture NAi is less than 0.3, preferably less than 0.2, and preferentially of the order of 0.1. These ranges of NAi values correspond approximately to opening angles ⁇ i of the illumination cone 20 less than 30°, preferably less than 20°, and preferentially of the order of 10°.
  • the source 2 is a laser diode making it possible to directly obtain the desired directivity and divergence for the incident light rays i.
  • the source 2 is an LED diode associated with a guiding structure making it possible to indirectly obtain the desired directivity and divergence for the incident light rays i.
  • the illumination cone 20 can therefore be formed directly from a laser diode or indirectly from an LED.
  • source 2 is the sun.
  • a particle present in channel 1 and passing through the illumination cone 20 will generate scattered light rays ii. These scattered light rays ii are re-emitted by the particle 10 symmetrically on either side of the optical axis (O) of the illumination cone 20, also called the optical axis of the source 2, as shown in Figures 7A And 7B .
  • the collection of the diffused light rays ii is advantageously done at the level of the optical inputs 41, 42, 43 of angular filtering devices 4a.
  • each angular filtering device 4a is associated with a photodetector 31, 32, 33 and makes it possible to angularly filter the light rays reaching this photodetector 31, 32, 33.
  • an angular filtering device 4a, 4b, 4c, 4d is preferably formed by an optical input 4x and a guide structure 4xy.
  • the optical inputs 41, 42, 43 of these angular filtering devices are arranged around the channel 1, so as to collect diffused light rays ii having different angles of incidence.
  • They can be arranged in a semicircle, from source 2 to an optical input diametrically opposite source 2, opposite source 2.
  • They can alternatively be arranged on a complete circle. They can also be arranged on two concentric circles, alternating or staggered, as illustrated below by other examples of realization. These choices may depend on the manufacturing costs, the size and the desired angular resolution for the detector.
  • the optical inputs may at least partially delimit channel 1, for example directly at a wall of channel 1.
  • they may be separated from the wall of channel 1. In this case, they may be covered by a protective or encapsulating layer so as to avoid fouling of said optical inputs.
  • the detector preferably comprises a filtering device 4a' whose optical input is aligned with the optical axis of the source 2, facing the source 2.
  • the photodetector associated with such an optical input advantageously makes it possible to carry out particle absorption measurements and/or drift checks of the source 2.
  • This optical input can also make it possible to collect a portion of the light rays not used for the angular analysis, for example incident light rays i not scattered by the particle 10. This collected portion can then be reinjected into the channel, either so as to maintain good brightness of the illumination cone 20, or so as to form another illumination cone, for example at a lower level of the channel. This makes it possible to limit the optical losses of the illumination cone 20. This ultimately makes it possible to benefit from a major portion of the light emitted by the source 2 for analysis purposes.
  • the optical inputs 41, 42, 43 preferably transmit the scattered light rays ii to the photodetectors 31, 32, 33 via guide structures.
  • These guide structures may be, for example, waveguides 411, 421, 431 as illustrated in figure 1 . As will be described in detail in reference to Figures 2 to 4A , these guiding structures can also be optical fibers 412, 422, 432, microlens systems 413 or even light traps 414, 424, 434.
  • Such a guiding structure is configured to transmit scattered light rays ii included in the collection cone 40 extending from the optical input associated with said guiding structure.
  • the NAc numerical aperture is less than 0.3, preferably less than 0.2, and preferably of the order of 0.1.
  • NAc values correspond approximately to opening angles ⁇ c of the collection cone 40 less than 30°, preferably less than 20°, and preferentially of the order of 10°.
  • NAc the numerical aperture of the guide structure.
  • NAc the numerical aperture of the guide structure.
  • NAc the numerical aperture of the guide structure.
  • a person skilled in the art will be able to determine the appropriate numerical aperture NAc, and produce guide structures having such a numerical aperture NAc.
  • the number of optical inputs and/or guiding structures arranged around the channel 1 is determined by the desired angular sampling. For example, for a distribution of the optical inputs and/or guiding structures on a semicircle, this number is preferably at least equal to ⁇ /2.arcsin (NAc).
  • the angular sampling carried out by the detector is symmetric.
  • the angular sampling is redundant and can be averaged. The noise affecting the angular analysis of the detector can thus be reduced.
  • the angular sampling carried out by the detector is asymmetric.
  • the angular sampling is non-redundant.
  • the angular resolution of the detector can thus be increased.
  • the intersection of the illumination cone 20 and a collection cone 40 makes it possible to define a useful volume V as illustrated in figure 1
  • the superposition of the useful volumes V makes it possible to define an analysis volume in which the diffusion of the particle 10 can be analyzed angularly by the detector.
  • the analysis volume is advantageously reduced. This allows spatial filtering for the position of the particles. This limits angular blur during the angular analysis of a particle flow.
  • the guide structures associated with the optical inputs 41, 42, 43 of the angular filtering devices 4a are linear waveguides 411, 421, 431.
  • These linear waveguides guide the scattered light rays ii collected at the corresponding optical inputs, mainly along their respective longitudinal axes.
  • Photodetectors 31, 32, 33 are positioned in the extension of the different longitudinal axes, preferably so that their photodetection surfaces are normal to the longitudinal axes.
  • the photodetectors can be coupled to their respective waveguides by direct coupling.
  • the angular resolution of the detector can be equated to ⁇ arcsin (NA).
  • the angular detection efficiency of such a detector is optimized.
  • the guide structures associated with the optical inputs 41, 42, 43 of the angular filtering devices 4b are optical fibers 412, 422, 432.
  • optical fibers 412, 422, 432 make it possible to guide the diffused light rays ii collected at the corresponding optical inputs 41, 42, 43 in particular along curvilinear paths.
  • optical axes at the inputs 41, 42, 43 of the optical fibers 412, 422, 432 coincide with radii of the cylinder forming the channel 1.
  • the photodetectors 31, 32, 33 are positioned at the output of the optical fibers 412, 422, 432, preferably on the same linear strip, or on the same matrix of photodetectors.
  • the photodetector array can be coupled to the optical fibers such that the photodetection surfaces of the photodetectors are normal to the optical axes at the output of the fibers.
  • the photodetector array can be coupled to the optical fibers edgewise, i.e. such that the photodetection surfaces of the photodetectors are parallel to the optical axes at the output of the fibers.
  • the output of the optical fibers may have an interface oriented according to an angle of total internal reflection so as to transmit the guided diffused light rays to the photodetection surfaces of the photodetectors.
  • a coupling network can be used to extract the scattered light rays ii guided in the fibers, to transmit them to the photodetection surfaces of the photodetectors.
  • the photodetectors may be separated from the guide structures, such that there is no contact between the photodetector surfaces of the photodetectors and these guide structures.
  • the photodetector strip of the detector can be easily changed. The maintenance of such a detector is therefore facilitated.
  • FIGS. 3A, 3B, 3C illustrate filtering devices having different collection and/or guiding structures which can be associated with the photodetectors and/or the light source 2.
  • FIG. 3A illustrates in longitudinal section a waveguide 411 comprising a core 4110 and a cladding 4111, mounted on a support 100.
  • the scattered light rays ii coming from the channel 1 and included in the collection cone 40 are collected at the optical input 41, guided by the waveguide 411 and transmitted to the photodetector 31.
  • Such a guiding structure formed by a waveguide is easily achievable using conventional micro-fabrication technologies.
  • FIG. 3B illustrates in longitudinal section a waveguide 411 comprising a core 4110 and a cladding 4111, mounted on a support 100.
  • the support 100 is configured to further receive an intermediate optical structure 51 between the channel 1 and the optical input 41.
  • This intermediate optical structure 51 preferably contributes to the shaping of the collection cone 40, for example so as to improve the angular resolution and/or detection sensitivity associated with the optical input considered.
  • This intermediate optical structure 51 can be configured to reduce the divergence of the collection cone 40, for example in the case of a waveguide with high index contrast. It can also widen a section S at the base of the collection cone 40, on the side of the entrance 41.
  • a microbead 51 for example made of a transparent polymer, having a diameter of between 10 and 500 ⁇ m can allow such shaping of the collection cone 40.
  • FIG. 3C illustrates in longitudinal section a ball, also called a microball, mounted on a support 100, directly associated with a photodetector 31.
  • This ball is directly configured to form at least part of the angular filtering device 4c.
  • the ball alone forms the angular filtering device 4c.
  • This ball therefore has an optical input 41 for collecting the scattered light rays ii included in the collection cone 40. It also allows these scattered light rays ii to be transmitted to the photodetector 31.
  • Such a collection structure formed by a ball is advantageously inexpensive.
  • the optical inputs associated with these collection and/or guidance structures preferably have a collection section S of a few tens of ⁇ m 2 , typically of the order of 40 ⁇ m 2 or even of the order of 100 ⁇ m 2 .
  • FIG. 5A to 5F schematically describe the production of a waveguide 411 of a detector according to the invention. This description can also be understood as the production of an optical fiber. More generally, the principle illustrated in these Figures 5A to 5F can be used to produce all or part of a detector according to the embodiments illustrated in Figures 1 to 3B .
  • a support 100 made of a semiconductor material such as silicon is provided. It may be thinned beforehand so as to maintain a thickness of support 100 of between 500 ⁇ m and 1 mm.
  • a first layer of a first optical polymer is deposited, preferably with a thickness of between 5 ⁇ m and 50 ⁇ m, so as to form the lower part of the cladding 4111 of the waveguide 411.
  • a second layer of a second optical polymer is deposited, preferably to a thickness of between 5 ⁇ m and 25 ⁇ m, so as to constitute the core 4110 of the waveguide 411 ( Figure 5A ).
  • This second optical polymer preferably has a refractive index higher than that of the first optical polymer, so as to obtain confinement by index contrast of the light rays transmitted by the waveguide 411.
  • This second optical polymer is chosen so as to have a low index contrast with the first polymer.
  • the numerical aperture of the waveguide is advantageously minimized.
  • the thicknesses of core 4110 and cladding 4111 are preferably chosen so that the waveguide 411 with low optical index contrast is configured to guide light propagating according to so-called extended optical modes, having for example transverse extension dimensions (relative to the propagation axis, or else relative to the optical axis of the waveguide) of several micrometers.
  • the core pattern of the 411 waveguide is then defined and/or etched by conventional lithography and/or etching methods ( Figure 5B ).
  • the second optical polymer constituting the core is a negative photosensitive optical resin of the SU-8 type conventionally used in the microelectronics industry.
  • the structuring of the core pattern of the waveguide can therefore be done solely by lithography, that is to say from an exposure step, preferably under UV radiation, followed by a development step, preferably with a liquid developer.
  • This pattern is then encapsulated by an encapsulation layer based on the first polymer so as to form the upper part of the sheath 4111 of the waveguide 411, complementary to the lower part ( Figure 5C ).
  • the upper portion preferably has a thickness substantially equal to the thickness of the lower portion.
  • this encapsulation layer may comprise a third optical polymer having a refractive index close to or substantially equal to that of the first optical polymer.
  • the 4111 sheath is thus completely formed.
  • an annealing step may be carried out so as to generate diffusion of the first and/or second optical polymer at heart wall level 4110 ( Figure 5D ). This diffusion advantageously improves the optical quality of the walls.
  • Channel 1 of the detector can then be etched through the cladding layers and/or the 4110 core.
  • Channel 1 is etched so as to form the optical input 41 of the waveguide 411 flush with said channel 1 ( Figure 5E ).
  • channel 1 is continued by a deep etching of the silicon support 100 ( Figure 5F ).
  • This method advantageously makes it possible to produce a plurality of polymer waveguides arranged in a base plane around a channel 1 in an inexpensive manner.
  • the waveguides may be based on ion-exchange doped glasses.
  • the waveguides may have a SiON-based core and a SiO2-based cladding.
  • the detector is in the form of a barrel 101 extending over a base plane ( Figure 4A ).
  • This barrel is not necessarily cylindrical, however.
  • This barrel 101 comprises a central, preferably cylindrical, through channel 1, an optical output 21 and a plurality of optical inputs 41, 42, 43 arranged along a first circle, called the collection circle, around and centered on the channel 1.
  • the plane in which the barrel 101 mainly extends is preferably perpendicular to the longitudinal axis of the channel 1.
  • the barrel 101 further comprises a plurality of housings 311, 321, 331, preferably cylindrical, arranged along a second circle, called the detection circle, of diameter greater than the diameter of the collection circle.
  • the detection circle is preferably centered on the channel 1.
  • the detection and collection circles are preferably concentric.
  • the cylindrical housings 311, 321, 331 are intended to receive the light source 2 and the photodetectors 31, 32, 33.
  • the barrel 101 further comprises a plurality of light traps 414, 424, 434 arranged in a star shape, along radii of the detection circle.
  • Each light trap 414, 424, 434 has an optical input 41, 42, 43 and forms, in part and preferably entirely, a 4d filtering device, as illustrated in Figure 4A .
  • a light trap is configured to transmit light rays in a low divergence beam, for example having a divergence angle of less than 15°.
  • Such a light trap may comprise a main optical axis along which light rays having a divergence angle relative to the optical axis of less than 15° are transmitted, and absorbing branches on either side of the main optical axis in which light rays having a divergence angle relative to the optical axis of greater than 15° are absorbed.
  • the absorbing branches are oriented according to the direction of propagation of the light rays, forming an acute angle with the optical axis of the light trap. They are configured to absorb the light rays propagating within them. Only light rays propagating mainly along the optical axis can thus pass through the light trap.
  • the cylindrical housing housing the light source 2 is connected to a “source” light trap having an optical output 21 and having a main axis oriented along a radius of the collection circle.
  • a cylindrical housing 311, 321, 331 housing a photodetector 31, 32, 33 is connected to a “photodetector” light trap 414, 424, 434 having an optical input 41, 42, 43 and a main axis oriented along a radius of the collection circle.
  • the absorbing branches of the “source” light trap and the absorbing branches of the “photodetector” light traps are oriented in opposite directions.
  • the light from exit 21 of the “source” light trap has a low divergence, regardless of the divergence of source 2 itself.
  • the light entering the optical inputs 41, 42, 43 is angularly filtered by the “photodetector” light traps 414, 424, 434, so that only a portion of the scattered light rays ii included in the collection cone 40 of each of the optical inputs 41, 42, 43 actually reaches the corresponding photodetectors 31, 32, 33.
  • Such a barrel 101 can advantageously be formed from a single material, for example silicon, without it being necessary to use transparent optical elements to filter and guide the light rays.
  • the photodetectors 31, 32, 33 can be arranged in the corresponding housings so that their respective photodetection surfaces 310, 320, 330 are included in the same plane parallel to the base plane, on a flat side of said cylindrical housings, for example at the bottom of these housings 311, 321, 331.
  • the source 2 can be arranged in the corresponding housing so that its emission surface is substantially included in this same plane parallel to the base plane, at the bottom of its housing.
  • Such an arrangement facilitates the integration of the photodetectors and the source into the detector.
  • the cylindrical housings 311, 321, 331 housing the photodetectors 31, 32, 33 preferably have reflective walls making it possible to reflect in all directions the diffused light rays ii reaching the entrances of the housings via the corresponding light traps, up to the photodetection surfaces 310, 320, 330.
  • the cylindrical housing is covered with a reflective and/or diffusing paint so as to obtain relatively uniform lighting inside the housing.
  • Such cylindrical housings advantageously form integral washers 311, 321, 331 making it possible to improve respectively the detection sensitivity and the illumination quality of the barrel detector.
  • the integrating washers can be replaced by integrating spheres.
  • the detector also includes a cover 102 for removing external stray light ( Figure 4B ).
  • This cover 102 is perforated in its center so as to form a passage towards channel 1.
  • the face of the cover 102 facing the cylindrical housings preferably comprises reflective surfaces at the level of these housings.
  • the cylindrical housings can be arranged in a staggered manner along two concentric detection circles of different radii.
  • the cylindrical housings 311, 321, 331 are therefore not necessarily equidistant from the channel 1.
  • the latter are arranged alternately on one circle and on the other.
  • This arrangement makes it possible to optimize the space requirement associated with cylindrical housings. Therefore, the distribution angle ⁇ between two successive photodetectors can be reduced. The angular resolution of the detector can be increased.
  • the housings located on the first circle and the housings located on the second circle may be located on either side of a median plane perpendicular to the longitudinal axis of the channel 1.
  • the optical inputs may be centered at the median plane, and prisms, guide structures and/or reflective surfaces may return or transmit the collected light rays to the photodetection surfaces of the photodetectors facing the median plane.
  • the distribution angle ⁇ can be constant along the detection circle(s), in particular between two successive photodetectors arranged outside the optical axis (O). This makes it possible to achieve symmetrical angular sampling by this detector, as illustrated in Figure 7A .
  • the distribution angle ⁇ can vary along the detection circle(s).
  • the cylindrical housings housing the photodetectors can be separated by a first distribution angle ⁇ 1 on a first half of the detection circle, and by a second distribution angle ⁇ 2, different from ⁇ 1, on the second half of the detection circle.
  • the first distribution angle ⁇ 1 can be of the order of 30° and the second distribution angle ⁇ 2 can be of the order of 36°. This makes it possible to achieve asymmetric angular sampling by this detector, as illustrated in FIG. Figure 7B .
  • the distribution angles ⁇ 1', ⁇ 2', ⁇ 3'... and/or the opening angles yc1, yc2, ⁇ c3, ⁇ c4... of the corresponding collection cones vary along the detection circle(s). It is thus possible to obtain a first type of sampling favoring the angular resolution, by example on a first half or on a first quarter of the detection circle on a side opposite to source 2, and a second type of sampling favoring sensitivity, that is to say the reduction of measurement noise, for example on a second half or on a second quarter of the detection circle on a side adjoining source 2.
  • a support 100 made of a semiconductor material such as silicon is provided. It may be thinned beforehand so as to maintain a thickness of support 100 of between 500 ⁇ m and 1 mm, preferably 750 ⁇ m.
  • a first lithography/etching step makes it possible to form the cylindrical housings 311, 321, 331, the light traps 414, 424, 434 and part of the channel 1.
  • the etching depth for this first step can be between 200 ⁇ m and 500 ⁇ m.
  • housings 311, 321, 331 and channel 1 are not completely drilled.
  • a second lithography/etching step then makes it possible to pierce the housings so as to accommodate the photodetectors 31, 32, 33 and the source 2, and the channel 1 so as to allow the passage of the fluid comprising the particles.
  • drilling can be done by laser micromachining.
  • the walls and bases of the integral washers are then covered with reflective and diffusing paint, for example by screen printing or by spraying using a solid stencil.
  • the cover 102 can be produced separately, from a thinned silicon substrate for example.
  • barrel 101 It is cut to the dimensions of barrel 101, drilled in its center at channel 1, and covered with reflective and diffusing paint on the areas intended to be opposite the housings of barrel 101.
  • the barrel 101 and the cover 102 are then assembled, for example by gluing.
  • the barrel and the cover are made at least partially of plastic and the assembly of the barrel and the cover is carried out by hot stamping.
  • the assembly is a thermoplastic weld.
  • the barrel and lid are made by 3D printing. They can be made in one piece. In this case, assembly may not be necessary.
  • the invention provides an effective solution for improving the angular resolution of the detector by limiting angular blur and/or measurement noise.
  • the detector may include multiple stacked barrels and/or multiple light sources. It may include both waveguide-type guiding structures and light trap-type guiding structures.

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Claims (12)

  1. Optischer Detektor für Partikel, umfassend mindestens:
    - einen zylindrischen Kanal (1) zum Empfangen eines Fluids, das mindestens ein Partikel (10) umfasst, und zum Empfangen mindestens eines einfallenden Lichtstrahls (i);
    - ein Erkennungssystem (3), das eine Vielzahl von Fotodetektoren (31, 32, 33) umfasst, wobei jeder Fotodetektor (31, 32, 33) Lichtstrahlen empfangen kann, die von dem Kanal (1) kommen und von dem mindestens einen Partikel (10) gestreut (ii) werden,
    der Detektor ferner ein Winkelfiltersystem (4) umfasst, das eine Vielzahl von Winkelfiltervorrichtungen (4a, 4b, 4c, 4d) umfasst, die jeweils mit einem Photodetektor (31, 32, 33) verbunden sind, wobei jede Winkelfiltervorrichtung (4a, 4b, 4c, 4d) so konfiguriert ist, dass sie die Lichtstrahlen (ii, iii, iv) aus dem Kanal (1) vor ihrem Empfang durch den Fotodetektor (31, 32, 33), mit dem sie verbunden ist, winkelmäßig filtert, wobei jede Winkelfiltervorrichtung (4a, 4b, 4c, 4d) einen optischen Eingang (41, 42, 43) mit einer numerischen Apertur umfasst, die kleiner als eine numerische Apertur des Photodetektors (31, 32, 33) ist, dem die Winkelfiltervorrichtung (4a, 4b, 4c, 4d) zugeordnet ist,
    wobei der Detektor dadurch gekennzeichnet ist, dass die optischen Eingänge (41, 42, 43) mindestens teilweise um den Kanal (1) herum verteilt sind, entlang mindestens eines Teils mindestens eines Kreises, wobei die Photodetektoren (31, 32, 33) entlang mindestens zwei konzentrischen Kreisen mit unterschiedlichen Radien versetzt angeordnet sind.
  2. Detektor nach dem vorstehenden Anspruch, wobei der optische Eingang (41, 42, 43) jeder Winkelfiltervorrichtung (4a, 4b, 4c, 4d) kleiner oder gleich 0,3 ist.
  3. Detektor nach einem der vorstehenden Ansprüche, wobei die Winkelfiltervorrichtung (4a, 4b, 4c, 4d) so konfiguriert ist, dass sie an ihrem optischen Eingang (41, 42, 43) einen Sammelkegel (40) definiert, wobei jeder Sammelkegel (40) einen Öffnungswinkel γc von weniger als 35° aufweist, um gestreute Lichtstrahlen (ii) mit Ausbreitungsrichtungen mit Einfallswinkeln, relativ zu einer optischen Achse des betreffenden optischen Eingangs (41, 42, 43), von weniger als 17,5° zu sammeln.
  4. Detektor nach einem der vorstehenden Ansprüche, wobei jeder optische Eingang (41, 42, 43) eine optische Achse aufweist, die mit einem Radius des Zylinders zusammenfällt, der den Kanal (1) bildet.
  5. Detektor nach einem der vorstehenden Ansprüche, wobei die Winkelfiltervorrichtung (4a, 4b, 4c, 4d) zwischen ihrem Eingang (41) und dem ihr zugeordneten Photodetektor (31) eine optische Führungsstruktur umfasst, die aus einer optischen Faser (412, 422, 432), einem Wellenleiter (411, 421, 431), einer Linse oder einer Lichtfalle (413, 423, 433) besteht.
  6. Detektor nach einem der vorstehenden Ansprüche, wobei die Photodetektoren (31, 32, 33) Photodetektoroberflächen (310, 320, 330) umfassen, die so angeordnet sind, dass sie sich in einer Ebene quer zu einer Längsachse des Kanals (1) befinden, wobei der Detektor ferner eine optische Integrationsstruktur umfasst, die so konfiguriert ist, dass sie die gestreuten Lichtstrahlen (ii), die an einem optischen Eingang (41, 42, 43) gesammelt werden, zu der Photodetektionsoberfläche (310) des Photodetektors (31) überträgt, der dem betreffenden optischen Eingang (41) zugeordnet ist, wobei die optische Integrationsstruktur zum Beispiel eine integrale Kugel, eine integrale Scheibe (311, 321, 331), ein Prisma ist.
  7. Detektor nach einem der vorstehenden Ansprüche, wobei der Kanal (1) zylindrisch ist und die optischen Eingänge (41, 42, 43) um den Kanal (1) auf Achsen in Verlängerung der Radien des Zylinders verteilt sind, wobei zwei aufeinanderfolgende Achsen durch einen Verteilungswinkel θ zwischen 15° und 45°, vorzugsweise in der Größenordnung von 30°, getrennt sind.
  8. Detektor nach dem vorstehenden Anspruch, wobei der Verteilungswinkel θ um den Kanal (1) herum variiert und wobei vorzugsweise ein erster Teil der optischen Eingänge (41, 42, 43) über eine erste Kreishälfte verteilt ist und einen ersten Verteilungswinkel θ1, zum Beispiel in der Größenordnung von 30°, aufweist, und wobei ein zweiter Teil der optischen Eingänge (41, 42, 43) über eine zweite Kreishälfte verteilt ist und einen zweiten Verteilungswinkel θ2 aufweist, der von θ1 unterschiedlich ist, zum Beispiel in der Größenordnung von 36°, um eine nicht-redundante Abtastung der gestreuten Lichtstrahlen (ii) zu erreichen.
  9. Detektor nach einem der vorstehenden Ansprüche, umfassend ferner für mindestens einige Filtervorrichtungen eine optische Zwischenstruktur (51) zwischen dem Kanal (1) und dem optischen Eingang (41, 42, 43), wobei die optische Zwischenstruktur (51) so konfiguriert ist, dass sie die Divergenz des Sammelkegels (40) verringert und/oder einen Abschnitt des Sammelkegels (40) des optischen Eingangs (41, 42, 43) erweitert, wobei die optische Zwischenstruktur (51) beispielsweise aus einer Mikrolinse und einer Mikrokugel ausgewählt wird.
  10. Verfahren zur Herstellung eines Detektors für Partikel nach einem der Ansprüche 1 bis 9, wobei das Verfahren mindestens die folgenden Schritte umfasst:
    - Bereitstellen eines Substrats,
    - Definieren der winkelförmigen Filtervorrichtungen (4a, 4b, 4c, 4d), die den Kanal (1) umgeben, auf einer Seite des Substrats,
    - Bilden des Kanals (1) durch das Substrat, um einen Durchgang für das Fluid zu ermöglichen,
    - Bilden der winkelförmigen Filtervorrichtungen (4a, 4b, 4c, 4d) an der Fläche des Substrats,
    - Verbinden eines Photodetektors (31, 32, 33) mit jeder Winkelfiltervorrichtung (4a, 4b, 4c, 4d).
  11. Verfahren nach dem vorstehenden Anspruch wobei die winkelförmigen Filtervorrichtungen (4d) Lichtfallen sind, die durch Ätzen des Substrats von der Substratfläche aus gebildet werden.
  12. Verfahren nach einem der beiden vorstehenden Ansprüche, das ferner die Bildung einer optischen Integrationsstruktur umfasst, die so konfiguriert ist, dass sie Lichtstrahlen von der Winkelfiltervorrichtung (4a, 4b, 4c, 4d) zu einer Photodetektionsoberfläche (310) des Photodetektors (31) überträgt, der der betreffenden Winkelfiltervorrichtung (4a, 4b, 4c, 4d) zugeordnet ist, die Photodetektionsoberfläche (310) sich hauptsächlich in Ebenen parallel zu der Substratfläche erstreckt, und die integrierende optische Struktur beispielsweise eine integrierende Scheibe (311, 321, 331) ist, die von der Substratfläche geätzt ist.
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US11221289B2 (en) 2022-01-11

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